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We show here that non-network metallopolymers can possess intrinsic microporosity stemming from contortion introduced by metallocene building blocks. Metallopolymers constructed from ferrocenyl building blocks linked by phenyldiacetylene bridges are synthesized and possess BET surface areas up to 400 m 2 g −1 . As solubility imparted by pendant groups reduces porosity, copolymerization is used to simultaneously improve both accessible surface area and solubility. Spectroscopic analysis provides evidence that mixed valency between neighboring ferrocenyl units is supported in these polymers. 

Abstract The optoelectronic properties of semiconducting polymers and device performance rely on a delicate interplay of design and processing conditions. However, screening and optimizing the relationships between these parameters for reliably fabricating organic electronics can be an arduous task requiring significant time and resources. To overcome this challenge, Polybot is developed—a robotic platform within a self‐driving lab that can efficiently produce organic field‐effect transistors (OFETs) from various semiconducting polymers via high‐throughput blade coating deposition. Polybot not only handles the fabrication process but also can conduct characterization tests on the devices and autonomously analyze the data gathered, thus facilitating the rapid acquisition of data on a large scale. This work leverages the capabilities of this platform to investigate the fabrication of OFETs using hydrogen bonding‐containing semiconducting polymers. Through high‐throughput fabrication and characterization, various data trends are analyzed, and large extents of anisotropic charge mobility are observed in devices. The materials are thoroughly characterized to understand the role of processing conditions in solid state and electronic properties of these organic semiconductors. The findings demonstrate the effectiveness of automated fabrication and characterization platforms in uncovering novel structure–property relationships, facilitating refinement of rational chemical design, and processing conditions, ultimately leading to new semiconducting materials. 

Abstract Durable and conductive interfaces that enable chronic and high‐resolution recording of neural activity are essential for understanding and treating neurodegenerative disorders. These chronic implants require long‐term stability and small contact areas. Consequently, they are often coated with a blend of conductive polymers and are crosslinked to enhance durability despite the potentially deleterious effect of crosslinking on the mechanical and electrical properties. Here the grafting of the poly(3,4 ethylenedioxythiophene) scaffold, poly(styrenesulfonate)‐b‐poly(poly(ethylene glycol) methyl ether methacrylate block copolymer brush to gold, in a controlled and tunable manner, by surface‐initiated atom‐transfer radical polymerization (SI‐ATRP) is described. This “block‐brush” provides high volumetric capacitance (120 F cm^─3), strong adhesion to the metal (4 h ultrasonication), improved surface hydrophilicity, and stability against 10 000 charge–discharge voltage sweeps on a multiarray neural electrode. In addition, the block‐brush film showed 33% improved stability against current pulsing. This approach can open numerous avenues for exploring specialized polymer brushes for bioelectronics research and application.